CN102154067A - Method for very quick and continuous preparation of biodiesel at room temperature - Google Patents
Method for very quick and continuous preparation of biodiesel at room temperature Download PDFInfo
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- CN102154067A CN102154067A CN2011100430881A CN201110043088A CN102154067A CN 102154067 A CN102154067 A CN 102154067A CN 2011100430881 A CN2011100430881 A CN 2011100430881A CN 201110043088 A CN201110043088 A CN 201110043088A CN 102154067 A CN102154067 A CN 102154067A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
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Abstract
The invention relates to a method for very quick and continuous preparation of biodiesel at room temperature. The method comprises the steps of: mixing isoamylol with tetrahydrofuran in proportion to generate a cosolvent A; mixing methanol with the cosolvent A in proportion to constitute denatured alcohol B; mixing the denatured alcohol B with lauryl sodium sulfate and sodium hydroxide in the proportion of 1:(1-10) to obtain a mixture C; simultaneously pumping raw material oil and the mixture C into a complete set of equipment D capable of quickly producing the biodiesel by a precise intelligent metering pump at certain speed for transesterification to obtain a semi-finished product E, and separating glycerol in the semi-finished product E to obtain crude biodiesel F and crude glycerol G; distilling and recovering the methanol and the cosolvent in the crude biodiesel F to obtain a finished product biodiesel H, wherein the recovered methanol and the recovered cosolvent in the step are introduced to a stock tank for recycling; and distilling and recovering the methanol and the cosolvent in the crude glycol G to obtain an industrial-grad glycol I, wherein the recovered methanol and the recovered cosolvent in the step are introduced to the stock tank for recycling. The method has the characteristics of simple reaction process, rapidness, high efficiency, low cost and the like.
Description
Technical field: the present invention relates to the preparation method of diesel oil, particularly a kind of room temperature extremely fast prepares method of bio-diesel oil continuously.
Background technology: the technology of domestic and international at present preparation biofuel has a variety of, mainly contains: chemical method, biological enzyme, supercritical methanol technology.Wherein the supercritical methanol technology speed of response is the fastest, but equipment making takes very costliness; The biological enzyme reaction times is very long, and enzyme costs an arm and a leg, the production cost height; Use chemical method the most generally, wherein chemical method respectively has characteristics according to the difference of catalyzer again.The invention belongs to chemical method, its ultimate principle is to utilize various types of alkali or acid catalyst, and lipid acid in the grease and glycerine group cutting and separating are opened, combine with methyl alcohol, carry out transesterification reaction, generate fatty acid methyl ester, the fatty acid methyl ester of generation is biofuel.But relate to concrete technology,, cause temperature of reaction, time, pressure etc. to differ greatly, thereby formed diversified patented technology because of catalyzer difference technology differs greatly.
Present technique is the patent of invention with one of the present patent application people, the patent No.: ZL 200510200025.7 denominations of invention: prepare method of bio-diesel oil and utility model patent fast, the patent No.: ZL 200920125900.3 denominations of invention: two technology of a kind of device of quick production biofuel are the basis, on the basis that utilizes two patented technologies, innovate and improve, be specially: the one, in reactant ratio, added suitable solubility promoter, make reactant become the homogeneity homogeneous phase by two-phase; The 2nd, make to be reflected in the patent No. ZL 200920125900.3 utility model patent devices and carry out.Thereby realized at room temperature can carrying out the biofuel chemical reaction, and improved speed of response 10-20 second greatly, and present technique is to operate under normal pressure.
At present, in existing numerous patented technologies, no matter be to use liquid soda acid or solid acid-base, its temperature of reaction is more than 60 ℃ invariably, and the reaction times also is at 60 minutes to 10 hours, and the reaction that has is still carried out under elevated pressures.This type of patent is more, and this place is not enumerated one by one, only enumerates with the similar application technology of the technology of the present invention to illustrate, to show difference.As:
1, application number is: 200610161635.5, and denomination of invention is: the method for continuous preparing biodiesel by solubilizer process in pipeline reactor.This patent and the technology of the present invention have similarity, but effect compare with present technique will be poor too much.Similarity is mainly has all added solubility promoter and has carried out in pipeline reactor.Difference is mainly reflected in this application patent temperature of reaction and still needs to carry out under 60-65 ℃, and the reaction times is 30-60 minute, and operation also is to carry out under normal pressure.And the application's patent temperature of reaction is between normal temperature 10-30 ℃, and the reaction times only needs 10-20 second, and operation is to carry out under normal pressure.We can say that the art of this patent is far away than this patent advanced person.This mainly is that the art of this patent is to innovate to form on the basis of a patent of invention and a utility model patent, and the better and more excellent factor of proportion scale of selected solubility promoter has caused present technique advanced more simultaneously.
2, the patent No. is: ZL200820081569.5, denomination of invention is: duct type prepares the device of biofuel continuously.This patent has realized the continuity of biofuel reaction, but belongs to utility model, and the chemical reaction condition that does not have in the invention creation patented technology supports.
3, application number is: 200910232276.1, and denomination of invention is: there is the preparation method of biofuel down in a kind of solubility promoter.This invention has used ethylene dichloride to be solubility promoter, but its reaction also needs to carry out under 45 ℃, and reaction is more than 1.5 hours.
4, application number is: 200710000084.9, and denomination of invention is: the method for producing biological diesel oil with single phase catalysis.This invention uses ritalin to be solubility promoter, and its temperature of reaction is 60-80 ℃, reaction times 1-2 hour.
Up to now, take a broad view of numerous patented technologies, do not find any bibliographical information and patented technology, can be simultaneously at normal temperature, normal pressure, continuously, prepare method of bio-diesel oil under the condition rapidly and efficiently.And present technique has dropped into THE INDUSTRIAL TRIAL at present, and it is stable to obtain product performance, and incendivity is good, can satisfy the normal use of various now diesel oil machineries well.
Summary of the invention: the object of the present invention is to provide a kind of room temperature extremely fast to prepare method of bio-diesel oil continuously, utilize this method can reach normal temperature, normal pressure, prepare the purpose of biofuel continuously, fast.
Formation of the present invention: the concrete operations step is poly-as follows:
A. primary isoamyl alcohol and tetrahydrofuran (THF) are pressed 3-7: the 7-3 mixed generates solubility promoter A;
B. methyl alcohol and A press 1-3: 1 mixed, form denatured alcohol B;
C. denatured alcohol B and sodium lauryl sulphate, sodium hydroxide are by 1: 1-10 mixes the mixture C that obtains;
D. raw oil material and C product are pressed certain speed simultaneously, pump into accurate intelligent metering pump among a kind of complexes D of quick production biofuel and carry out transesterification reaction, get work in-process E, wherein, raw oil material is 100 with the material speed ratio that the C product are controlled by the intelligent metering pump: 15-30;
E. separate the glycerine among the work in-process E, get coarse biodiesel F and raw glycerine G;
F. methyl alcohol and the solubility promoter among the coarse biodiesel F reclaimed in distillation, gets refined biometric diesel oil H, methyl alcohol that this is partially recycled and solubility promoter, and incoming stock jar recycles;
G. methyl alcohol and the solubility promoter among the raw glycerine G reclaimed in distillation, gets technical grade glycerine I, methyl alcohol that this is partially recycled and solubility promoter, and incoming stock jar recycles;
H. in the 4th step d operation, from the intelligent metering pump material is pumped into the device D, come out from efficient pipeline reactor to material, only need 10-20 second, this promptly is the time of transesterification reaction, and reaction is to carry out under room temperature 10-30 ℃, normal pressure.
Its raw oil material is an animal-plant oil, as: jatropha curcasl oil, Euphorbia lathyris oil, Oleum Tiglii, Fructus Zanthoxyli oil, Chinese pistache seed wet goods vegetables oil and tenebrio molitor wet goods animal oil are raw material.
Compared with the prior art, the present invention has following characteristics: innovation part of the present invention is two patented technologies and solubility promoter have been carried out integrated, makes production of biodiesel technology produce creationary breakthrough, mainly shows following several respects:
1. transesterification reaction is carried out under room temperature 10-30 ℃.Neither need heating, also do not need refrigeration, greatly reduce the energy consumption in the production, numerous patented technologies all need to heat the situation that just can carry out transesterification reaction before having changed.
2. the saponification phenomenon can not take place in the production process, thoroughly done away with side reaction.It is an incidental side reaction in the production of biodiesel process that the saponification phenomenon takes place, and this side reaction occurring generally is to take place easily when temperature is higher, and the present invention carries out at normal temperatures, then saponification reaction can not take place.
3. speed of response is exceedingly fast, and transesterification reaction only needs 10-20 second (not comprising the aftertreatment time) to finish.Numerous patented technology transesterification reaction times all will shorten the reaction times greatly 60 minutes to 10 hours situation before having changed, and have improved production efficiency.
4. facility investment is little, and because of transesterification reaction is to carry out under normal temperature, normal pressure, the equipment making expense is not high.The present invention makes the production technique of biofuel reach at room temperature, normal pressure, extremely fast and under the condition of serialization carry out by the integrated innovation to several technology, makes production technique simpler, easy to operate.
Embodiment:
Embodiment 1:
Jatropha curcasl oil (the southwest of Guizhou Province Condar forestry science and technology company limited provides) with state, the southwest of Guizhou Province output is a raw material, and its physical and chemical index is: 1. proportion 930g/L; 2. viscosity 42mm
2/ s (40 ℃); 3. outward appearance is a brown; 4. acid number 0.5mgKOH/g.Producing the step gathers as follows:
1, with pump the 312L primary isoamyl alcohol is pumped into raw material storage tank with the 313L tetrahydrofuran (THF) and mix, generate the solubility promoter A of 625L.
2, with pump 938L methyl alcohol is pumped into the catalyst dissolution jar with 625L solubility promoter A and mix, get 1563L denatured alcohol B.
3, catalyzer 25kg is put in the catalyst dissolution jar, uses the denatured alcohol B that obtains of step and stir and dissolve, the C product.
4, with 5000kg jatropha curcasl raw oil material with the speed of accurate intelligent metering pump with 25.00L/min, the C product are pressed the speed of 7.26L/min, pump into simultaneously to use among the device D that manufactures and designs by ZL 200920125900.3 patents to carry out transesterification reaction.
5, about 10-20 is after second, and reaction mass promptly comes out from efficient pipeline reactor, obtains work in-process E this moment.
6, the glycerine among the separation work in-process E gets coarse biodiesel F and raw glycerine G.
7, methyl alcohol and the solubility promoter among the coarse biodiesel F reclaimed in distillation, gets refined biometric diesel oil H.Methyl alcohol that this is partially recycled and solubility promoter, incoming stock jar recycles.
8, methyl alcohol and the solubility promoter among the raw glycerine G reclaimed in distillation, gets technical grade glycerine I.Methyl alcohol that this is partially recycled and solubility promoter, incoming stock jar recycles.
Gained biofuel in the present embodiment, through chemical examination, its index such as following table:
Table one jatropha curcasl oil biodiesel index
| Test item | Technical requirements | Detected result | Conclusion |
| Sulphur content/(%) (m/m) | ≤0.05 | 0.01 | Qualified |
| Acid number/(mgKOH/g) | ≤0.80 | 0.20 | Qualified |
| Copper corrosion (50 ℃, 3h)/(level) | ≤1 | 1 | Qualified |
| Kinematic viscosity (40 ℃)/(mm 2/s) | 1.9～6.0 | 4.5 | Qualified |
| Condensation point/(℃) | ≤0 | 0 | Qualified |
| Cold filter clogging temperature/(℃) | ≤-4 | -6 | Qualified |
| Flash-point (remaining silent)/(℃) | ≥130 | 136 | Qualified |
| Cetane value | ≥50 | 55 | Qualified |
| Density (20 ℃)/(kg/m 3) | 820～900 | 876 | Qualified |
| Mechanical impurity | Do not have | Do not have | Qualified |
| Moisture/(%) (V/V) | Vestige | Vestige | Qualified |
Embodiment 2:
With Euphorbia lathyris oil (have another name called money, state, the southwest of Guizhou Province tropical crops institute provides) is raw material, and its physical and chemical index is: 1. proportion 920g/L; 2. viscosity 34mm
2/ s (40 ℃); 3. outward appearance black; 4. acid number 0.86mgKOH/g.Producing the step gathers as follows:
1, with pump the 100L primary isoamyl alcohol is pumped into raw material storage tank with the 87L tetrahydrofuran (THF) and mix, generate the solubility promoter A of 187L.
2, with pump 220L methyl alcohol is pumped into the catalyst dissolution jar with 187L solubility promoter A and mix, get 407L denatured alcohol B.
3, catalyzer 12kg is put in the catalyst dissolution jar, uses the denatured alcohol B that obtains of step and stir and dissolve, the C product.
4, with 1500kg Euphorbia lathyris raw oil material with the speed of accurate intelligent metering pump with 18.00L/min, the C product are pressed the speed of 4.57L/min, pump into simultaneously to carry out transesterification reaction in the device among the D.
5, after about 10～20 seconds, reaction mass promptly comes out from efficient pipeline reactor, obtains work in-process E this moment.
6, the glycerine among the separation work in-process E gets coarse biodiesel F and raw glycerine G.
7, methyl alcohol and the solubility promoter among the coarse biodiesel F reclaimed in distillation, gets refined biometric diesel oil H.Methyl alcohol that this is partially recycled and solubility promoter, incoming stock jar recycles.
8, methyl alcohol and the solubility promoter among the raw glycerine G reclaimed in distillation, gets technical grade glycerine I.Methyl alcohol that this is partially recycled and solubility promoter, incoming stock jar recycles.
Gained biofuel in the present embodiment, through chemical examination, its index such as following table:
Table two Euphorbia lathyris oil biodiesel index
| Test item | Technical requirements | Detected result | Conclusion |
| Sulphur content/(%) (m/m) | ≤0.05 | 0.01 | Qualified |
| Acid number/(mgKOH/g) | ≤0.80 | 0.16 | Qualified |
| Copper corrosion (50 ℃, 3h)/(level) | ≤1 | 1 | Qualified |
| Kinematic viscosity (40 ℃)/(mm 2/s) | 1.9～6.0 | 4.1 | Qualified |
| Condensation point/(℃) | ≤0 | -4 | Qualified |
| Flash-point (remaining silent)/(℃) | ≥130 | 142 | Qualified |
| Cold filter clogging temperature/(℃) | ≤-4 | -8 | Qualified |
| Density (20 ℃)/(kg/m 3) | 820～900 | 870 | Qualified |
| Mechanical impurity | Do not have | Do not have | Qualified |
| Moisture/(%) (V/V) | Vestige | Vestige | Qualified |
With tenebrio molitor grease (Shandong Agricultural University provides) is raw material, and its physical and chemical index is: 1. proportion 935g/L; 2. viscosity 39mm
2/ s (40 ℃); 3. outward appearance is faint yellow, has and solidifies fatty acid ester on a small quantity; 4. acid number 0.91mgKOH/g.Producing the step gathers as follows:
1, first pre-treatment tenebrio molitor grease, the little fat acid esters that the condensation filtering separation is fallen to solidify gets tenebrio molitor stock oil.
2, with pump the 10L primary isoamyl alcohol is pumped into raw material storage tank with the 13L tetrahydrofuran (THF) and mix, generate the solubility promoter A of 23L.
3, with pump 45L methyl alcohol is pumped into the catalyst dissolution jar with 23L solubility promoter A and mix, get 68L denatured alcohol B.
4, catalyzer 3.20kg is put in the catalyst dissolution jar, uses the denatured alcohol B that obtains of step and stir and dissolve, the C product.
5, the tenebrio molitor grease after 400kg is handled is with the speed of accurate intelligent metering pump with 13.00L/min, and the C product are pressed the speed of 2.60L/min, pump into simultaneously to carry out transesterification reaction in the device among the D.
6, after about 10～20 seconds, reaction mass promptly comes out from efficient pipeline reactor, obtains work in-process E this moment.
7, the glycerine among the separation work in-process E gets coarse biodiesel F and raw glycerine G.
8, methyl alcohol and the solubility promoter among the coarse biodiesel F reclaimed in distillation, gets refined biometric diesel oil H.Methyl alcohol that this is partially recycled and solubility promoter, incoming stock jar recycles.
9, methyl alcohol and the solubility promoter among the raw glycerine G reclaimed in distillation, gets technical grade glycerine I.Methyl alcohol that this is partially recycled and solubility promoter, incoming stock jar recycles.
Gained biofuel in the present embodiment, through chemical examination, its index such as following table:
Table three tenebrio molitor biofuel detects index
| Test item | Technical requirements | Detected result | Conclusion |
| Sulphur content/(%) (m/m) | ≤0.05 | 0.02 | Qualified |
| Acid number/(mgKOH/g) | ≤0.80 | 0.30 | Qualified |
| Copper corrosion (50 ℃, 3h)/(level) | ≤1 | 1 | Qualified |
| Kinematic viscosity (40 ℃)/(mm 2/s) | 1.9～6.0 | 4.4 | Qualified |
| Condensation point/(℃) | ≤0 | -2 | Qualified |
| Cold filter clogging temperature/(℃) | ≤-4 | -4 | Qualified |
| Flash-point (remaining silent)/(℃) | ≥130 | 135 | Qualified |
| Density (20 ℃)/(kg/m 3) | 820～900 | 878 | Qualified |
| Mechanical impurity | Do not have | Do not have | Qualified |
| Moisture/(%) (V/V) | Vestige | Do not have | Qualified |
Embodiment 4:
With Fructus Zanthoxyli oil (the southwest of Guizhou Province Condar forestry science and technology company limited provides) is raw material, and its physical and chemical index is: 1. proportion 918g/L; 2. viscosity 35mm
2/ s (40 ℃); 3. outward appearance is an aterrimus; 4. acid number 0.89mgKOH/g.
Producing the step gathers as follows:
1, with pump the 100L primary isoamyl alcohol is pumped into raw material storage tank with the 90L tetrahydrofuran (THF) and mix, generate the solubility promoter A of 190L.
2, with pump 200L methyl alcohol is pumped into the catalyst dissolution jar with 190L solubility promoter A and mix, get 390L denatured alcohol B.
3, catalyzer 13kg is put in the catalyst dissolution jar, uses the denatured alcohol B that obtains of step and stir and dissolve, the C product.
4, with the 1000kg Fructus Zanthoxyli oil with the speed of accurate intelligent metering pump with 18.00L/min, the C product are pressed the speed of 4.57L/min, pump into simultaneously to carry out transesterification reaction in the device among the D.
5, after about 10～20 seconds, reaction mass promptly comes out from efficient pipeline reactor, obtains work in-process E this moment.
6, the glycerine among the separation work in-process E gets coarse biodiesel F and raw glycerine G.
7, methyl alcohol and the solubility promoter among the coarse biodiesel F reclaimed in distillation, gets refined biometric diesel oil H.Methyl alcohol that this is partially recycled and solubility promoter, incoming stock jar recycles.
8, methyl alcohol and the solubility promoter among the raw glycerine G reclaimed in distillation, gets technical grade glycerine I.Methyl alcohol that this is partially recycled and solubility promoter, incoming stock jar recycles.
Gained biofuel in the present embodiment, through chemical examination, its index such as following table:
Table five Semen Pericarpium Zanthoxyli biofuel detects index
| Test item | Technical requirements | Detected result | Conclusion |
| Sulphur content/(%) (m/m) | ≤0.05 | 0.01 | Qualified |
| Acid number/(mgKOH/g) | ≤0.80 | 0.30 | Qualified |
| Copper corrosion (50 ℃, 3h)/(level) | ≤1 | 1 | Qualified |
| Kinematic viscosity (40 ℃)/(mm 2/s) | 1.9～6.0 | 4.0 | Qualified |
| Condensation point/(℃) | ≤0 | -1 | Qualified |
| Cold filter clogging temperature/(℃) | ≤-4 | -6 | Qualified |
| Flash-point (remaining silent)/(℃) | ≥130 | 137 | Qualified |
| Cetane value | ≥50 | 59 | Qualified |
| Density (20 ℃)/(kg/m 3) | 820～900 | 875 | Qualified |
| Mechanical impurity | Do not have | Do not have | Qualified |
| Moisture/(%) (V/V) | Vestige | Do not have | Qualified |
Claims (2)
1. a room temperature extremely fast prepares method of bio-diesel oil continuously, it is characterized in that: the concrete operations step is poly-as follows:
A. primary isoamyl alcohol and tetrahydrofuran (THF) are pressed 3-7: the 7-3 mixed generates solubility promoter A;
B. methyl alcohol and A press 1-3: 1 mixed, form denatured alcohol B;
C. denatured alcohol B and sodium lauryl sulphate, sodium hydroxide are by 1: 1-10 mixes the mixture C that obtains;
D. raw oil material and C product are pressed certain speed simultaneously, pump into accurate intelligent metering pump among a kind of complexes D of quick production biofuel and carry out transesterification reaction, get work in-process E, wherein, raw oil material is 100 with the material speed ratio that the C product are controlled by the intelligent metering pump: 15-30;
E. separate the glycerine among the work in-process E, get coarse biodiesel F and raw glycerine G;
F. methyl alcohol and the solubility promoter among the coarse biodiesel F reclaimed in distillation, gets refined biometric diesel oil H, methyl alcohol that this is partially recycled and solubility promoter, and incoming stock jar recycles;
G. methyl alcohol and the solubility promoter among the raw glycerine G reclaimed in distillation, gets technical grade glycerine I, methyl alcohol that this is partially recycled and solubility promoter, and incoming stock jar recycles;
H. in the 4th step d operation, from the intelligent metering pump material is pumped into the device D, come out from efficient pipeline reactor to material, only need 10-20 second, this promptly is the time of transesterification reaction, and reaction is to carry out under room temperature 10-30 ℃, normal pressure.
2. room temperature according to claim 1 extremely fast prepares method of bio-diesel oil continuously, it is characterized in that: its raw oil material is an animal-plant oil, as: jatropha curcasl oil, Euphorbia lathyris oil, Oleum Tiglii, Fructus Zanthoxyli oil, Chinese pistache seed wet goods vegetables oil and tenebrio molitor wet goods animal oil are raw material.
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| CN2011100430881A CN102154067A (en) | 2011-02-23 | 2011-02-23 | Method for very quick and continuous preparation of biodiesel at room temperature |
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| CN2011100430881A CN102154067A (en) | 2011-02-23 | 2011-02-23 | Method for very quick and continuous preparation of biodiesel at room temperature |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108219982A (en) * | 2016-12-22 | 2018-06-29 | 内蒙古中细软技术开发有限公司 | Novel cosolvent method biodiesel synthesis |
-
2011
- 2011-02-23 CN CN2011100430881A patent/CN102154067A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108219982A (en) * | 2016-12-22 | 2018-06-29 | 内蒙古中细软技术开发有限公司 | Novel cosolvent method biodiesel synthesis |
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Application publication date: 20110817 |